تفاعل #46067

معادلة التفاعل

Sodium hydride

Trifluoroacetamide

ammonium chloride

E-1,3-dichloropropene

→

N-(3-Chloro-allyl)-2,2,2-trifluoro-acetamide

المذيبات

THF

water

ظروف التفاعل

المعالجة

1. 1
   أخرىthe temperature of the reaction with a water bath
2. 2
   workup.WAITAfter 2 min.
3. 3
   درجة الحرارةthe reaction was heated
4. 4
   درجة الحرارةto reflux for 45 min
5. 5
   درجة الحرارةThe mixture is then cooled to room temperature
6. 6
   أخرىThe mixture is transferred to a separatory funnel
7. 7
   استخلاصextracted with ether (2×400 mL)
8. 8
   تجفيفThe combined organic layers were dried (MgSO4)
9. 9
   تركيزconcentrated under reduced pressure
10. 10
    أخرىto obtained a colorless oil that

الإجراء التجريبي

Trifluoroacetamide (10.44 g, 92.4 mmol) is dissolved in THF (30 mL). Sodium hydride (60% weight dispersion in mineral oil, 3.1 g, 77 mmol) is then added in small portions at room temperature while regulating the temperature of the reaction with a water bath. The mixture is stirred at room temperature for 5 min., after which E-1,3-dichloropropene (4.5 mL, 49.4 mmol) is added. After 2 min., the mixture thickened, and the reaction was heated to reflux for 45 min. The mixture is then cooled to room temperature, and saturated aqueous ammonium chloride (20 mL) and water (40 mL) are added. The mixture is transferred to a separatory funnel and extracted with ether (2×400 mL). The combined organic layers were dried (MgSO4) and concentrated under reduced pressure to obtained a colorless oil that was used for the next step.

المصدر